Process for the manufacture of amids of higher fatty acids.



0. A. H. HfKUSTERS & L. OTTEMANN.

moonss FOR THE MANUFAGTUBE 0F mms 01-" HIGHER FATTY ACIDS.

9 1 5 ,680 BPEOIIEFS.

APPLICATION FILED FEB. 8, 1908.

Patented Mar. 16, 1909.

i STATES "mari st;

OSCAR AUGUST HUBERT HUGO xosrnnsjor HEMEL'INGEN,

Y, :nannemennmnrq AND, Louis QTTEMANN, or

PROCESS I on THE um mc momm s Onaiermnfarrfadrhsy No. 915,380. orignin application'fledlarch 29, 1901,

To all it mag concern:

Be it known that we, Oscan AUGUsT HU- BERT HUGO Kos'rnns, a resident of Hemelin on, Germany, and LOUIS OTTEMANN, a resi ent of Bremen, Germany, both subjects of the Emperor of Germany, have jointly invented certain new and useful Improvements'in Processes for the Manufacture of Amids of the Higher Fatty Acids, of whicha tendency to decompose the amids produced. Moreover this Water, which remains in the vessel during the entire process, is,

detrimental particularly, as it exerts a pressure of from 25 to 30 atmospheres (at the temperature em loyed), and this pressure is further increase when the ammonium salts of the fatty acids are heated, by the liberated ammonia; the consequence is that very strong apparatus is required for carrying, out

The term i the process above referred to. higher fatty acids as used herein is applied to fatty acids containing at least six carbon atoms.

Our present invention avoids the defects just mentioned, and consists, briefly described, in heating the higher fatty acids in a closed vessel under regulatable pressure in the presence of gaseousammonia.

plained. I

The ap aratus comprises a suitable closed vessel a or instance, a digester), connected with the delivery port of a pump 0 by a pipe 1) extending almost to the bottom. of the vessel. From the cover (1 a pipe. e leads to a drying chamber or tower f of any suitable construction, which by pipes 9, his connected with the suction port of the pum c. A branch pi e i connects the pi es 9, i with a cylinder containing liqui ammonia; a three-way cock m is preferably located at the junction of the pipes g, h, t. 'A circulating path is thus provided the pump ownthat amids of the higher,

This process for the pro-- e accompanying drawing illustrates in a. diagrammatic manner, an apparatus suitable for carrying out our process hereafter exe The first reaction a mes otLottorn Batont. thu er-E mira, 19cc.

semi No. 865,247. Divided and an; application filed February a, 1908. Serial No. 414,905. (Specimens) i through pipe I) to'vessel .a, thence throu h pipe. e todrying'chamberf, and back' to t e pump through pipes g, it. Any suitabledrying agent,isuch'- as caustic-hme, may bexused in the chamber f. The vessel 0 isheated in any suitable manner, for instance, as shown,

by means of a furnace in which it is set.

The operation is as follows The vessel a of a'ca acity-(of say 300 liters) is filled with a suitab e amount (say 100 kilograms) of a higher fatty acid, such as stearic acid, and

heated to the proper temperature for instance 190 centigrade. 'Thereupon, the

pump 0 is set in motion and the cock m as .well as the discharge valve of-fthe receptacle la are opened, so as to allow the liquid ammoniato escape in gaseous form into the pipes 11, h and to pass into the heated mass contained in the vessel a. This gas, which is dry, is supplied in greater amount than is necessary for the reaction. An amid and water are formed by the action of the amrnonia gas on the heated fatty acid, said water being carried away a'svapor with the excess of ammonia gas passing to the'drying chamber g through the pipe e. The drying agent in the chamber f absorbs'such water, so that dry ammonia gas returns to the pump .0 through the pipes g,*h. The deficiency caused by the combination of the ammonia with the fatty acid, is supplied by the admission of new gas from the receptacle 7c. The

pressure maintained in. the apparatus during the reaction may be about two atmospheres or less, and the lprocess is completed in about three ,hours. he ammonia first forms an ammonium salt with the fatty acid, and

from this ammonium-salt the amid of the "fatty acid is formed; both reactions, 'however, are practically simultaneous.

may be expressed by the equation: a"

C H COOH +-NH,-= C H, COONH Stearlo acid. Ammonia. *Stearate or ammonium.

Stearate 01 ammonium. Stearic amid. Water-t.

One of the reat advantages of our method consists in t e immediate. removal of ithe reaction water from the heated vessel;

another important advantage is the fact that the pressure'within the digester is independent of the temperature employed. Since the ammonia gas travels in a continuous path or cycle, and is dried before it returns to the vessel a, a perfect utilization of the gas is secured, and therefore a very economical Working.

This ap lication is a division of one filed by us in the United States Patent Office on March 29, 1907, Serial No.365, 247.

We claim as our invention:

l. The process of roducing amids of the higher fatty acids, w 'ch consistsin heating the said acids in a closed vessel in the presence of ammonia gas, and withdrawing the excess of ammonia gas together with any water formed during the reaction.

2. The process of roducing amids of the higher fatty acids, w ich consists in heating the saidacids in a closed vessel inthe presence of ammonia gas, withdrawing the excess of ammonia gas together. with any water formed during the reaction, drying such withdrawn ammonia .gas, and returning it into contact with the fatty acid.

In testimony whereof, we have hereunto signed our names in the presence of two subscribing witnesses.

OSCAR, AUGUST HUBERT HUGO KilSTERS. LOUIS OT'IEMANN. Witnesses: v

' FREDERICK HOYERMA'NN. FERDINAND Rnron. 

